CN116429488B - Method for inverting in-situ micro-regional chronology history of heterogeneous mineral and application - Google Patents
Method for inverting in-situ micro-regional chronology history of heterogeneous mineral and application Download PDFInfo
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- 238000000095 laser ablation inductively coupled plasma mass spectrometry Methods 0.000 claims description 28
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- 229910052845 zircon Inorganic materials 0.000 claims description 22
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims description 22
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- UXBZSSBXGPYSIL-UHFFFAOYSA-N phosphoric acid;yttrium(3+) Chemical compound [Y+3].OP(O)(O)=O UXBZSSBXGPYSIL-UHFFFAOYSA-N 0.000 description 1
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Abstract
The application provides a method for inverting the chronology history of heterogeneous minerals in situ micro-regions and application thereof, which realizes the separation and purification of target minerals by carrying out data analysis, extraction, enhancement and other treatments on original scan data, and simultaneously highlights the annual indexes (U content, pb content and Pb) in the target mineral phase by applying a noise data processing technology 206 /U 238 Ratio of Pb 207 /U 235 Ratio, th/U ratio), the distribution characteristics of the fixed-year minerals are displayed more intuitively, the fixed-year favorable positions and the crystal growth change trend of the fixed-year minerals are displayed more intuitively, and a fine point position design and more accurate definition are provided for later high-precision fixed-year analysisThe heterogeneous mineral crystal growth process is subjected to several geological events, so that the mineral formation history is inverted, researches such as mineralogy, mineral geochemistry, mineralogy and the like are better developed, and the heterogeneous mineral crystal growth process is a novel indispensable auxiliary means for mineralogy and an auxiliary mineral exploration method.
Description
Technical Field
The application belongs to the technical field of mineral evolution history research, and particularly relates to a method for inverting the in-situ micro-regional chronology history of heterogeneous minerals and application thereof.
Background
In the course of geological research, the era of accurately measuring the formation of geologic bodies has become an indispensable method for knowing the history of formation thereof. However, the geologic body is affected by various internal and external factors during or after formation, and thus the composition heterogeneity of the mineral crystal is changed. Such as diffusion, recrystallization, secondary growth, erosion reprecipitation, etc., can affect the element content and the change of the U-Pb isotope system of the minerals. Therefore, how to accurately define the geological significance represented by the U-Pb isotope on the submicron scale in the minerals is important to recovering the evolution history experienced by the geologic body.
With the progress of in-situ analysis technology, laser ablation-inductively coupled plasma mass spectrometry (LA-ICP-MS) plays an important role in the aspect of in-situ microcell dating, and the technology is simple, convenient and quick, has the characteristics of low operation cost and the like, but the LA-ICP-MS point analysis has randomness and blindness, and the formation process of highly non-uniform samples is difficult to accurately limit, so that important dating information is lost. The spatial distribution of elemental and isotopic composition is the most critical step in characterizing the mineral growth process and history, and is an important aspect in determining whether multi-stage and multi-secondary growth is present. Therefore, more and more students begin to use LA-ICP-MS technology to perform scan analysis (MAPPING) on minerals and the like, and through the work, distribution conditions of elements, isotopes and the like on the surfaces of the minerals can be well obtained, but compared with LA-ICP-MS point analysis, the LA-ICP-MS point analysis has low precision due to the characteristics of shallow ablation depth, short ablation time, short analysis time and the like, noise data (such as negative values and empty values) can be generated in the process of collecting signals and testing, and in addition, the scan analysis can complete analysis on symbiotic minerals, cracks, inclusion and the like of the tested minerals in the process of testing, and the analysis can cause interference on the tested minerals.
Therefore, a new and efficient method suitable for U-Pb dating in-situ micro-regions of uranium-containing heterogeneous minerals is needed to be found, namely, the method has the accuracy of point analysis, and the distribution of mineral elements and isotopes in space can be well reflected, so that the mineral formation history can be accurately inverted, and important limits are provided for formation and evolution of geologic bodies.
Disclosure of Invention
The application aims at providing a method for inverting the in-situ micro-regional chronology history of heterogeneous minerals and application thereof aiming at the defects of the prior art.
In order to achieve the above purpose, the present application adopts the following technical scheme:
the application provides a method for inverting the chronology history of heterogeneous mineral in-situ micro-regions, which comprises the following specific steps:
s1, collecting a bedrock sample, wherein the bedrock sample is rich in any one of zircon, rutile or garnet;
step S2, sample lithology analysis
S21, grinding the collected bedrock sample into a probe sheet with the width of 25mm, the length of 30-35mm and the thickness of 0.05mm, a laser sheet with the width of 25mm, the length of 30-35mm and the thickness of 0.08mm, observing the corresponding mineral characteristics under a microscope, and recording the lithology and symbiotic combination characteristics of the mineral characteristics in detail;
s22, selecting single mineral crystals with good crystal forms, complete particles and no impurity inclusion as representative samples;
s23, designing a rectangular area which is larger than the particle size of a single mineral crystal on a bedrock sample by taking the single mineral crystal as a target, marking the rectangular area by using a marker pen, and carrying out MAPPING analysis on the element surface scanning of an in-situ micro-area of a laser ablation inductively coupled plasma mass spectrometer on the selected experimental test position;
step S3, mineral phase separation and purification of MAPPING data
The matrix data of LA-ICP-MS MAPPING obtained in the step 23 is subjected to K-means semi-automatic supervision multi-channel classification method to realize mineral phase separation and purify single mineral crystals;
step S4, data cleaning and filtering analysis
The high U minerals are subjected to data cleaning by utilizing purified and separated high U mineral data, negative numbers and null values are replaced, median filtering is performed on the processed data, and element distribution rules are highlighted;
low U mineral, cleaning data with purified and separated low U mineral data, replacing negative value and null value, median filtering the processed data, and determining high U 238 Low Pb 204 A component endless belt of (a);
step S5, period discrimination and SPOT point location design
High U minerals: making U-Pb age harmonic graph by using the filtered data, determining whether multiple times and Pb loss exist, calculating relation between Th/U and Pb loss, and determining U 238 The area with stable element distribution is used as the area for designing LA-ICP-MS SPOT analysis point positions, and U is eliminated 238 Designing an element mutation or gradual change region, and designing a LA-ICP-MS SPOT analysis point location distribution diagram according to the principle;
low U minerals: searching high U and low Pb component ring bands, judging whether multiple times exist, and determining the number of times of U 238 Designing a LA-ICP-MS SPOT analysis point position distribution diagram in a region with stable element distribution and content more than 10 ppm;
step S6, accurately defining the age of mineral formation
High U minerals: processing and interpreting the fixed year data by using ICPMSDataCal software, and combining with ISOPLOTR software to manufacture a U-Pb age harmony map and a U-Pb weighted average age map;
low U minerals: processing and interpreting data using ICPMSDataCal software, if., single point Pb 206 /U 238 The age harmony is greater than 80%, and the U-Pb age harmony map and the U-Pb weighted average age map can be manufactured by using ISOPLOTR software. If single point Pb 206 /U 238 Age harmony is mostly less than 80%, and T-W U-Pb harmony age illustrations can be made using ISOPLOTR software.
Further, in step S22, the single mineral crystal particle size is greater than 0.1mm.
Further, in step S2, the laser ablation inductively coupled plasma mass spectrometer is composed of Agilent 7900 quadrupole plasma mass spectrometry, COMPexPro 102arf 193nm excimer laser and micro las optical system, and uses a mineral established standard sample and an international standard substance glass standard sample NIST610 as correction standards to perform U-Pb isotope dating and trace element content processing, and uses iolite4 software to perform data reduction and derive matrix data of MAPPING elements.
Further, the test parameters of the laser ablation inductively coupled plasma mass spectrometer comprise laser working parameters and ICP-MS working parametersParameters, the laser working parameters are as follows: in the laser ablation process, high-purity helium is used as carrier gas, high-purity argon is used as compensation gas to adjust sensitivity, the carrier gas and the high-purity argon are mixed through a T-shaped joint before entering plasma, surface scanning MAPPING is adopted in the early stage, the sampling mode is rapid point ablation, a point is connected with a line to form a surface, each analysis point lasts for 3-5 s, the time comprises 1-2 s blank signal, 2-3 s sample ablation and cleaning time, the helium flow is 0.6-0.9L/min, and the laser energy density is 1.5J/cm 2 The diameter of the laser beam spot is 5-10 mu m, the frequency is 10Hz, and the scanning speed is 3-6 mu m/s; the ICP-MS working parameters are as follows: the RF radio frequency power is 1550w, the plasma gas flow rate is 15L/min, the sampling depth is 2-5 mu m, the integration time is 2-5 s, and the auxiliary argon flow is 1.0L/min.
Further, SPOT analysis SPOT is adopted in the later stage, the sampling mode is SPOT ablation, each analysis point lasts for 70-90 s, the time comprises a blank signal of 15-20 s, a sample ablation signal of 40s and a cleaning time of 15-20 s, the helium flow is 0.8L/min, the laser energy is 80mJ, the laser beam SPOT diameter is 32-60 mu m, the frequency is 2-8 Hz, and the pulse number is 90-200 times; the ICP-MS working parameters are as follows: the RF power is 1550w, the plasma gas flow rate is 15L/min, the sampling depth is 5-5.5 mu m, the integration time is 40s, and the auxiliary argon flow is 1.0L/min.
Further, in step S3, MATLAB software is used to perform the K-means semi-automatic supervised multi-channel classification.
Further, in step S3, the phase separation of minerals refers to data separation of different minerals by the content of the principal element of the measured minerals, wherein the principal element of the measured minerals is an element with a content of more than 5wt.%, only the minerals of the definite year are left, other minerals are proposed, and finally the obtained two-dimensional matrix image is obtained.
Further, in step S4, in the specific implementation process of the data cleaning and filtering analysis, the high U minerals perform data cleaning by using purified and separated high U mineral data, the negative number and the null value are replaced by 0.1 times of the minimum value, the processing data are subjected to median filtering by using the mineral mapping software, and then the matrix data are converted into two-dimensional element images by using XMapTools software, so that the element distribution rule is highlighted.
Further, in step S4, the low U minerals are subjected to data cleaning by using the purified and separated low U mineral data, the negative value and the null value are replaced by 0 values, the processed data are subjected to median filtering by using the mineral mapping software, and then the matrix data are converted into two-bit element images by using the XMapTools software, so that the high U is determined 238 Low Pb 204 Is a component annulus of (a).
A second object of the present application is to provide the use of the above method of inverting the in situ micro-regional chronology history of heterogeneous minerals in mineral exploration.
Compared with the prior art, the technical scheme provided by the application has the beneficial effects that:
(1) According to the method for inverting the in-situ micro-regional chronology history of the heterogeneous mineral, disclosed by the application, the separation and purification of the target mineral are realized by carrying out data analysis, extraction, enhancement and other treatments on original scan data, meanwhile, the noise data processing technology is applied, the distribution characteristics of the annual indexes (U content, pb206/U238 ratio, pb207/U235 ratio and Th/U ratio) in the target mineral phase are highlighted, the annual beneficial parts, the annual potential and the crystal growth change trend of the annual mineral are displayed more intuitively, a fine point position design is provided for the later high-precision point analysis and the annual analysis, the geological events of the heterogeneous mineral are more accurately limited, so that the formation history of the mineral is inverted, and researches on mineralogy, mineralogy geochemistry, mineralogy and the like are better developed, and the method is a new indispensable auxiliary means and method for mineralogy.
(2) According to the method, the target minerals are accurately separated and purified by using a nonlinear smoothing filtering technology through a K-means semiautomatic supervision multichannel classification model, so that the relation between the scan data and the point data is established, the realization of the step can be realized through software MineralMAPPING, the application of the scan data in the in-situ micro-regional annual of heterogeneous minerals is realized, the scan data and the point data are enhanced, and the method has very strong practical and research values in the fields of mineralogy, mineral deposit science, earth science and the like.
(3) The method provided by the application realizes the phase separation and purification of heterogeneous definite-year ores;
(4) The scanning analysis of the target minerals is realized, and the annual indexes in the target minerals are enhanced;
(5) The capability of judging the fixed-year mineral period and the precision of setting the high-precision fixed-year point location are improved;
(6) The in-situ micro-area annual level of the heterogeneous mineral is improved, and the mineral crystal evolution history and the like are more accurately inverted;
(7) The method for inverting the in-situ micro-regional chronology histories of the heterogeneous minerals can enhance the geological information of the scanning data, more conveniently highlight the chronology information of the minerals in definite years and invert the diagenetic mineral formation histories, and has stronger research significance and practical value.
Drawings
FIG. 1 is a plot of a favorable plot of Qidamu basin north delineation samples;
FIG. 2 is a diagram of rutile probe tile and subsurface lithology characteristics for the Lv Liang mountain area;
FIG. 3 shows the scan data set (a-c) and mineral phase separation effect (d) for classification of example 1;
FIG. 4 is a graph of the purified sweep data resampling and data preprocessing of example 1;
FIG. 5 is a component bin of high U238 low Pb204 after median filtering in example 1;
FIG. 6 is a schematic diagram of the multiple-period forming annulus and SPOT point location of the rutile isotope ratio scan of example 1;
FIG. 7 is a graph showing the results of LA-ICP-MS SPOT analysis data in example 1;
FIG. 8 is a plot of the high accuracy U-Pb age harmonic (a) and the weighted average age (b) of the rutile multiphasic SPOT of example 1;
FIG. 9 is a diagram of a zircon probe tile in the green beam mountain area;
FIG. 10 is a MAPPING dataset (a-c) and mineral phase separation effect (d) for classification of example 2;
FIG. 11 is a chart of resampling and preprocessing of the MAPPING data after purification in example 2;
FIG. 12 is a graph of the component bins for high U238 low Pb204 after median filtering in example 2;
FIG. 13 is a schematic representation of zircon isotope ratio MAPPING multiple-phase forming annulus and SPOT SPOT designs;
FIG. 14 is a schematic representation of zircon isotope ratio MAPPING multiple passes to form an annulus, pb loss, and SPOT SPOT;
FIG. 15 is a graph showing the results of LA-ICP-MS SPOT analysis data in example 2;
FIG. 16 is a plot of zircon multi-stage SPOT high precision U-Pb age harmonics.
Detailed Description
No particular technique or condition is identified in the present application, which is performed according to techniques or conditions described in the literature in this field or according to the product specifications. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Technical terms and parameters related to the application
(1) K-means semi-automatic supervised multi-channel classification: the method is a cluster analysis algorithm for iterative solution, and comprises the steps of dividing data into K groups, randomly selecting K objects as initial cluster centers, calculating the distance between each object and each seed cluster center, and distributing each object to the cluster center nearest to the object. The cluster centers and the objects assigned to them represent a cluster. For each sample assigned, the cluster center of the cluster is recalculated based on the existing objects in the cluster. This process will repeat until a certain termination condition is met. The termination condition may be that no (or a minimum number of) objects are reassigned to different clusters, no (or a minimum number of) cluster centers are changed again, and the sum of squares of errors is locally minimum. K-means algorithm definition distance metric d ij Indicating that sample i and sample j are at a distance ofTo represent a squared euclidean distance; where p is the dimension of the data itself (typically two-dimensional). The K value is determined in combination with the actual situation, wherein in order to distinguish the research mineral from other minerals, oneThe K value is typically chosen to be 2, and the center of each class is recalculated using a defined loss function with constant iterative convergence. Wherein the loss function is defined as the sum of the distances between the sample and the center of the class to which it belongs: />Wherein->Is the center of the class.
(2) High U minerals and low U minerals: here we set the threshold value of U content to 200ppm, i.e. the minerals with U content > =200ppm are defined as high U minerals, such as zircon, monazite, xenotime, etc.; minerals with a U content of 1-200 ppm are defined as low U minerals such as rutile, apatite, garnet, etc.
(3) Multiple times: the term "multi-stage" refers to the presence of relatively significant amounts of U, pb and Pb in heterogeneous minerals 206 /U 238 Ratio of Pb 207 /U 235 Ratio, th/U ratio, etc. And judging that the mineral has undergone a plurality of formation events by comparing the relation between the element content and the ratio, and inverting the mineral formation history.
(4) Median filtering: the method is a nonlinear signal processing technology capable of effectively suppressing noise based on a sequencing statistical theory, and the principle is that the value of one point in a digital image or a digital sequence is replaced by the median value of each point value in a neighborhood of the point, so that surrounding pixel values are close to each other, and isolated noise points are eliminated. The method is to remove a two-dimensional sliding template with a certain structure, sort pixels in the plate according to the pixel value, calculate the median value and replace. The two-dimensional median filter output is g (x, y) =med ({ f (x-k, y-l), (k, l e W) }), where f (x, y), g (x, y) are the original signal and the processed signal, respectively. W is a two-dimensional template, generally a 3*3 area, and parameters of the template can be adjusted according to the situation.
(5) U-Pb age harmonic diagram: namely Pb 206 /U 238 -Pb 207 /U 235 A graph, according to the inverse calculation ratio of the known ages, the point is cast to obtain a curve representing the ages with the same agesThe diagram of the U-Pb system, i.e., the harmony line, is called a harmony diagram, and the specific pattern is shown in the examples.
(6) U-Pb weighted average age plot: by Pb 206 /U 238 Age (t) i ) And its error (s t i ]) Data according to t Average of ＝Σ(t i /s[t i ] 2 )/Σ(1/s[t i ] 2 ) The formula calculates the weighted average age and stores Pb 206 /U 238 Age (t) i ) And its error (s t i ]) The data are presented as a box plot, i.e., a U-Pb weighted average age plot. The magnitude of the weighted average age is not only dependent on the magnitude of the change between the ages of the individual zircons, but also on the number of occurrences of each zircon age, and typically data with a degree of synergy of less than 80% is not used, for example.
(7) T-W U-Pb harmonic age scheme: namely Pb 206 /U 238 -Pb 207 /Pb 206 And (3) a coordinate graph, namely a track formed by different time harmonics and age points is called a Tera-Wasserburg harmonic curve. On this curve, the degree of harmony with respect to a young mineral can be displayed more sufficiently, and the age of the lower intersection is generally taken as the age of formation of the mineral.
The MineralMAPPING software used in the application is independently developed by the inventor, and the copyright registration certificate of the computer software is 2020SR0341873.
The scanning MAPPING analysis used in the application is completed by adopting a laser ablation inductive coupling plasma mass spectrometer, the laser ablation inductive coupling plasma mass spectrometer consists of an Agilent 7900 quadrupole plasma mass spectrum, a COMPexPro 102ArF 193nm excimer laser and a micro Las optical system, a mineral established standard sample and an international standard substance glass standard sample NIST610 are used as correction standards, U-Pb isotope dating and microelement content processing are carried out, and data reduction is carried out by using iolite4 software and matrix data of MAPPING elements are derived.
The test parameters of the laser ablation inductively coupled plasma mass spectrometer comprise laser working parameters and ICP-MS working parameters, wherein the laser working parameters are as follows: in the laser ablation process, high-purity helium is used as carrier gas, high-purity argon is used as compensation gas to adjust sensitivity, the high-purity helium and the high-purity argon are mixed through a T-shaped joint before entering plasma, the sampling mode is point ablation, each analysis point lasts for 70 seconds, the sampling mode comprises blank signals of 15-20 seconds, sample ablation signals of 40 seconds and cleaning time of 15-20 seconds, the helium flow is 0.8L/min, the laser energy is 80mJ, the laser beam spot diameter is 44 mu m, the frequency is 5Hz, and the pulse number is 300 times; the ICP-MS working parameters are as follows: the RF radio frequency power is 1550w, the plasma gas flow rate is 15L/min, the sampling depth is 5-5.5 mm, the integration time is 40s, and the auxiliary argon flow is 1.0L/min.
The laser ablation system was equipped with a signal smoothing device for this analysis of laser beam spots and step sizes of 5 μm by 5 μm for a period of 3s per spot. In the U-Pb isotope setting and trace element content treatment, a mineral established standard sample (for example, a 91500 standard sample for zircon) and a glass standard substance NIST610 are adopted as external standards to respectively carry out isotope and trace element fractionation correction. Later, the data is restored by the iolite4 software and matrix data of MAPPING elements are derived.
Example 1
Inversion of low U heterogeneous mineral in situ micro-regional chronology history
(1) The system collects the data of the existing stratum, structure, magma rock and the like in the north edge of the Qida basin, comprehensively analyzes the research potential of the data, and researches and delineates a favorable sampling area, namely a green beam mountain research area, as shown in figure 1.
(2) And (5) selecting a green beam mountain area, and collecting a surface spodumene, namely a long english vein sample. During the sampling process, the following information is recorded in real detail, as shown in table 1:
table 1.
(3) The collected sample is ground into a probe sheet and a laser sheet, the microscopic lithology characteristics of the rutile are observed under a microscope, and the optical characteristics, symbiotic combination and special phenomena of the rutile are described and recorded in detail. Gold red with representative characteristics is selected, a marker pen is used for ensuring accurate circle position on a probe sheet or a laser sheet, the record number is recorded (shown in figure 2), and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) in-situ micro-area element surface scanning (MAPPING) analysis is carried out on the selected experimental test position.
(4) Fe, nb and Sn elements in LA-ICPMS scanning data are selected as classification basis (shown in figures 3a-3 c), a K-means semi-automatic supervision multi-channel classification method is adopted, the classification quantity is set to be two types, the separation of rutile from other minerals is realized, and rutile crystals are purified (shown in figure 3 d).
(5) Resampling and replacing negative and null values (as shown in fig. 4) with purified and isolated rutile data, median filtering the processed data to determine high U 238 Low Pb 204 The component zones (shown in FIG. 5) of (a) provide for single mineral component discrimination and LA-ICP-MS point of analysis (SPOT) point of design.
(6) Searching high U and low Pb and Pb 206 /U 238 Ratio and Pb 207 /U 235 The ratio component zones were determined to be multiple times (fig. 6a-6 c), the LA-ICP-MS SPOT analysis SPOT profile was designed (fig. 6 d), and SPOT experimental testing was performed. The LA-ICP-MS SPOT analysis data results are shown in FIG. 7.
(7) Processing and interpreting data using icpmsdata cal software to find a single point Pb 206 /U 238 Age concordance was greater than 80%, so U-Pb age concordance (as shown in FIG. 8 a) and U-Pb weighted average age (as shown in FIG. 8 b) were plotted using ISOPLOTR software. Therefore, two-phase U element enrichment is found in the rutile crystal growth process, the Ma is highly enriched at an early stage 428, and the enrichment degree of the Ma is reduced at 426 along with the crystal growth, so that the in-situ micro-regional chronology history of the heterogeneous mineral (rutile) is finely inverted.
Example 2
Inversion of high U heterogeneous mineral in situ micro-regional chronology history
(1) The system collects the data of the existing stratum, structure, magma rock and the like in the north edge of the Qida basin, comprehensively analyzes the research potential of the data, and researches and delineates a favorable sampling area, namely a green beam mountain research area (shown in figure 1).
(2) And (5) selecting a green beam mountain area, and collecting a surface spodumene, namely a long english vein sample. During the sampling process, the following information is recorded in real detail, as shown in table 2 below:
table 2.
(3) The collected samples were ground into probe and laser chips (as shown in fig. 9), and microscopic lithology characteristics of zircon were observed under a microscope to describe and record the optical characteristics, symbiotic combinations, and special phenomena of zircon in detail. Zircon with representative characteristics is selected and a marker is used for ensuring accurate zircon mineral circle positions on a probe sheet or a laser sheet, the number is recorded, and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) in-situ micro-area element surface scanning (MAPPING) analysis is carried out on the selected experimental test positions.
(4) Hf, ti and Zr in LA-ICP-MS MAPPING data are selected as classification basis (fig. 10a-10 c), a K-means semi-automatic supervision multi-channel classification method is adopted, classification quantity is set to be two, separation of zircon from other minerals is achieved, and zircon crystals are purified (fig. 10 d).
(5) Resampling and replacing negative and null values (as shown in FIG. 11) with purified and isolated zircon data, median filtering the processed data to determine high U 238 Low Pb 204 The component zones (shown in fig. 12) of (a) are shown, the element zone information is highlighted, and preparation is provided for single mineral component discrimination and LA-ICP-MS point (SPOT) analysis point design.
(6) Making U-Pb age harmonic diagram (shown in figure 13) by using filtered data, and searching for high U, low Pb and Pb 206 /U 238 Ratio and Pb 207 /U 235 The ratio component zones (shown in fig. 14a-14 b) were determined whether there were multiple periods and Pb loss (shown in fig. 14a-14 b), and the relationship between Th/U and Pb loss was calculated (shown in fig. 14 c), and LA-ICPMS SPOT analysis point distribution plots (shown in fig. 14d-14 e) were designed and SPOT experimental tests were performed. The LA-ICP-MS SPOT analysis data results are shown in FIG. 15.
(7) The data were processed and interpreted using ICPMSDataCal software and a U-Pb age harmonic plot (as shown in fig. 16) and a U-Pb weighted average age plot were made using ISOPLOTR software. Therefore, it was found that zircon had a multi-stage secondary crystal growth phenomenon, a zircon core formed around 439Ma and formed in an environment of high U/Th ratio, and a zircon rim formed around 426Ma and formed in an environment of low U/Th ratio as zircon crystals grew, in which Pb loss phenomenon was caused by a later geological event, which was detrimental to zircon age determination, and heterogeneous mineral (zircon) in-situ micro-regional chronology history and formation conditions were finely inverted by this method.
The embodiments described above and features of the embodiments herein may be combined with each other without conflict.
The foregoing description of the preferred embodiments of the application is not intended to limit the application to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the application are intended to be included within the scope of the application.
Claims (8)
1. A method for inverting the chronology history of heterogeneous minerals in situ micro-regions, comprising the steps of:
s1, collecting a bedrock sample, wherein the bedrock sample is rich in any one of zircon, rutile or garnet;
step S2, sample lithology analysis
S21, grinding the collected bedrock sample into a probe sheet with the width of 25mm, the length of 30-35mm, the thickness of 0.05mm, the width of 25mm, the length of 30-35mm and the thickness of 0.08mm, observing the corresponding mineral characteristics under a microscope, and recording the lithology and symbiotic combination characteristics of the mineral characteristics in detail;
s22, selecting single mineral crystals with good crystal forms, complete particles and no impurity inclusion as representative samples;
s23, designing a rectangular area which is larger than the particle size of a single mineral crystal on a bedrock sample by taking the single mineral crystal as a target, marking the rectangular area by using a marker pen, and carrying out MAPPING analysis on the element surface scanning of an in-situ micro-area of a laser ablation inductively coupled plasma mass spectrometer on the selected experimental test position;
step S3, mineral phase separation and purification of MAPPING data
The matrix data of LA-ICP-MS MAPPING obtained in the step 23 is subjected to K-means semi-automatic supervision multi-channel classification method to realize mineral phase separation and purify single mineral crystals;
step S4, data cleaning and filtering analysis
The method comprises the steps of (1) carrying out data cleaning on high U minerals by using purified and separated high U mineral data, replacing negative numbers and null values with 0.1 times of minimum values, carrying out median filtering on processed data by using Minalamapping software, and then converting matrix data into two-dimensional element images by using XMAPTools software to highlight element distribution rules;
the method comprises the steps of (1) carrying out data cleaning on low-U minerals by using purified and separated low-U mineral data, replacing negative values and null values with 0 values, carrying out median filtering on processed data by using MineralMAPPING software, and then converting matrix data into two-bit element images by using XMAPTools software to determine component endless belts of high U238 and low Pb 204;
step S5, period discrimination and SPOT point location design
High U minerals: making a U-Pb age harmonic graph by using the filtered data, determining whether multiple periods and Pb loss exist, calculating the relation between Th/U and Pb loss, taking a region with stable U238 element distribution as a region for designing LA-ICP-MS SPOT analysis point positions, excluding a U238 element mutation or gradual change region, and designing a LA-ICP-MS SPOT analysis point position distribution map according to the principle;
low U minerals: searching a component ring belt with high U and low Pb, judging whether the component ring belt has multiple periods, and designing a LA-ICP-MS SPOT analysis point position distribution diagram for a region with stable U238 element distribution and content more than 10 ppm;
step S6, accurately defining the age of mineral formation
High U minerals: processing and interpreting the fixed year data by using ICPMSDataCal software, and combining with ISOPLOTR software to manufacture a U-Pb age harmony map and a U-Pb weighted average age map;
low U minerals: processing and interpreting data by using ICPMSDataCal software, and if the single-point Pb206/U238 age harmony is more than 80%, making a U-Pb age harmony map and a U-Pb weighted average age map by using ISOPLOTR software; if the single point Pb206/U238 age harmony is mostly less than 80%, the T-W U-Pb harmony age illustration can be made using ISOPLOTR software.
2. The method of claim 1, wherein in step S22, the single mineral crystal particle size is greater than 0.1mm.
3. The method of claim 1, wherein in step S2, the laser ablation inductively coupled plasma mass spectrometer is composed of Agilent 8900 quadrupole plasma mass spectrometry, COMPexPro 102ArF 193nm excimer laser and micro las optical system, and the U-Pb isotope dating and trace element content processing is performed using mineral standard samples and international standard substance glass standard samples NIST610/NIST612 as calibration standards, and data reduction is performed using iolite4 software and matrix data of MAPPING elements is derived.
4. The method of claim 3, wherein the test parameters of the laser ablation inductively coupled plasma mass spectrometer include a laser operating parameter and an ICP-MS operating parameter, the laser operating parameter being: in the laser ablation process, high-purity helium is used as carrier gas, high-purity argon is used as compensation gas to adjust sensitivity, the carrier gas and the high-purity argon are mixed through a T-shaped joint before entering plasma, surface scanning MAPPING is adopted in the early stage, the sampling mode is rapid point ablation, a point connecting line is used, a line is used for forming a surface, each analysis point lasts for 3-5 s, the time comprises 1-2 s blank signal, 2-3 s sample ablation and cleaning time, the helium flow is 0.6-0.9L/min, the laser energy density is 1.5J/cm < 2 >, the laser beam spot diameter is 5-10 mu m, the frequency is 10Hz, and the scanning speed is 3-6 mu m/s; the ICP-MS working parameters are as follows: the RF power is 1550w, the plasma gas flow rate is 15L/min, the sampling depth is 2-5 mu m, the integration time is 2-5 s, and the auxiliary argon flow is 1.0L/min.
5. The method of claim 4, wherein the post-stage SPOT analysis SPOT is performed in a SPOT ablation mode, each analysis SPOT lasts for 70-90 s, and comprises a blank signal of 15-20 s, a sample ablation signal of 40s and a cleaning time of 15-20 s, wherein the helium flow is 0.8L/min, the laser energy is 80mJ, the laser beam SPOT diameter is 32-60 μm, the frequency is 2-8 Hz, and the pulse number is 90-200 times; the ICP-MS working parameters are as follows: the RF power is 1550w, the plasma gas flow rate is 15L/min, the sampling depth is 5-5.5 mu m, the integration time is 40s, and the auxiliary argon flow rate is 1.0L/min.
6. The method of claim 5, wherein in step S3, MATLAB software is used to semi-automatically supervise multi-channel classification of the K-means.
7. The method according to claim 6, wherein in step S3, the mineral phase separation refers to data separation of different minerals by the measured principal element content of the minerals, wherein the principal element of the measured minerals is an element with a content of more than 5 wt%, only the minerals of definite years are left, other minerals are proposed, and the finally obtained two-dimensional matrix image is obtained.
8. Use of the method of any one of claims 1-7 in mineral exploration.
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